CN107557618B - Low-resistance temperature-sensitive high-conductivity heat-resistant aluminum alloy and preparation process and application thereof - Google Patents

Low-resistance temperature-sensitive high-conductivity heat-resistant aluminum alloy and preparation process and application thereof Download PDF

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CN107557618B
CN107557618B CN201710760344.6A CN201710760344A CN107557618B CN 107557618 B CN107557618 B CN 107557618B CN 201710760344 A CN201710760344 A CN 201710760344A CN 107557618 B CN107557618 B CN 107557618B
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aluminum alloy
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CN107557618A (en
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李红英
赵守鑫
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Central South University
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Abstract

The invention discloses a low-resistance temperature-sensitive high-conductivity heat-resistant aluminum conductor and a preparation process and application thereof, belonging to the technical field of new electrical materials. The conductor mainly comprises Al, Fe, Zr, Hf, Yb and inevitable impurity elements, the raw materials of the conductor comprise industrial pure aluminum with the purity of 99.70% and intermediate alloy containing corresponding alloy elements, and the corresponding aluminum alloy blank is obtained by smelting, refining, casting and heat treatment. The obtained aluminum alloy blank has the electric conductivity of more than 60 percent IACS at 20 ℃, the electric conductivity of more than 40 percent IACS at 150 ℃, the electric conductivity of more than 36 percent IACS at 200 ℃ and the tensile strength of more than 70 MPa. After 80% cold deformation, the heat-resistant temperature of the obtained aluminum alloy blank is not lower than 200 ℃ for a long time (400h) and not lower than 250 ℃ for a short time (1 h). The obtained aluminum alloy can be used as at least one of a guide rod, a bus bar and a lead.

Description

Low-resistance temperature-sensitive high-conductivity heat-resistant aluminum alloy and preparation process and application thereof
Technical Field
The invention relates to a low-resistance temperature-sensitive high-conductivity heat-resistant aluminum alloy subjected to composite microalloying and composite heat treatment, and a preparation process and application thereof, and belongs to the technical field of new electrical materials.
Background
Aluminum has good conductive performance, and can be widely applied to the fields of transmission lines, transformer substations, aluminum electrolysis, buildings and the like as a conductor material. Pure aluminum has high conductivity, but has low strength and poor heat resistance, and microalloying can improve the heat resistance and strength, but has a very adverse effect on the conductivity.
For electrical aluminum, the national standard GB/T30552-0)[1+α(T~T0)]Where ρ (T)0) Is a certain reference temperature T0(typically 20 ℃) temperature coefficient of resistance αThe smaller the sensitivity of the resistivity to the temperature is, the higher the conductivity can be kept at a certain temperature, and the electric energy loss of the high-temperature-service-life-span solar cell can be reduced.
The inventor makes more beneficial attempts in the aspect of developing a high-conductivity heat-resistant aluminum alloy wire in the early period, for example, in patent CN201610177708.3, an iron-added light-weight high-conductivity heat-resistant aluminum wire is disclosed, which mainly comprises Al, B, Zr, Fe and La, and has high room-temperature conductivity and strength, and the short-time heat-resistant temperature reaches 230 ℃, but the patent does not relate to high-temperature conductivity, does not grasp the change rule of the conductivity along with the temperature rise, and is difficult to apply to occasions with high service temperature.
The invention comprehensively regulates and controls the conductivity and heat resistance of the alloy by the composite microalloying of Yb, Zr, Hf and other elements and the cooperation of a composite heat treatment system, obtains the high-conductivity heat-resistant aluminum alloy with low resistance and temperature sensitivity, and can keep certain conductivity and strength at higher temperature, namely has better high-temperature conductivity and heat resistance. When the aluminum alloy developed and designed by the invention is used at a higher temperature, the electric energy loss can be obviously reduced due to the relatively small amplitude of the electric conductivity reduction, which has important significance for energy conservation and emission reduction.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the aluminum alloy with reasonable component proportion, high conductivity, heat resistance and low resistance temperature sensitivity, and the preparation process and the application thereof.
The invention relates to a low-resistance temperature-sensitive high-conductivity heat-resistant aluminum alloy, which comprises the following alloy elements in percentage by mass:
Zr:0.01~0.10%;
Hf:0.01~0.10%;
Yb:0.05~0.20%;
Fe:0.05~0.15%;
the mass ratio of Yb to Zr is more than 1, the total content of Zr and Hf is less than or equal to 0.15%, the content of impurity Si is less than 0.05%, and the total content of impurities Ti, V, Cr, Mn and the like is less than 0.01%. The total content of impurity elements is less than 0.06%.
Preferably, the aluminum alloy comprises the following components in percentage by mass:
Zr:0.05~0.10%;
Hf:0.01~0.05%;
Yb:0.10~0.20%;
Fe:0.08~0.15%;
the mass ratio of Yb to Zr is more than 1, the total content of Zr and Hf is less than or equal to 0.15%, the content of impurity Si is less than 0.05%, the total content of impurities Ti, V, Cr, Mn and the like is less than 0.01%, and the balance is Al.
As a further preferable scheme, the aluminum alloy comprises the following components in percentage by mass:
Zr:0.05~0.10%;
Hf:0.01~0.03%;
Yb:0.10~0.20%;
Fe:0.09~0.12%;
the mass ratio of Yb to Zr is more than 1, the total content of Zr and Hf is less than or equal to 0.13%, the content of impurity Si is less than 0.05%, the total content of impurities Ti, V, Cr, Mn and the like is less than 0.01%, and the balance is Al.
Zr, Hf and Fe are transition group elements which greatly impair the electrical conductivity of the alloy, particularly when they exist in a solid solution state. The invention fully exerts the synergistic effect of the Yb, Zr, Hf and Fe elements by the composite addition of trace alloy elements and the special two-stage aging process, and produces unexpected effects.
In the present invention, the total content of Zr and Hf is in the range of 0.06 to 0.15 wt%, preferably 0.06 to 013 wt%; the mass ratio of Yb to Zr is greater than 1, preferably 1.5 or greater, more preferably 1.5 to 5, and still more preferably 1.5 to 2. By reasonably controlling the ratio of Yb to Zr and the total content of Zr and Hf and combining a two-stage aging process of low temperature first and high temperature second, the induced desolventizing and coarsening inhibition effects among elements are fully exerted, and Al with the grain diameter less than 50nm is formed as shown in figures 1(a) to 1(c)3(Hf, Zr, Yb) composite particles having Al as the core3Yb phase, Zr and Hf elements are richIs concentrated in Al3An outer layer of Yb phase. Yb has higher diffusion rate in aluminum alloy, and Al with fine dispersion distribution can be precipitated when heat treatment is carried out in a lower temperature range3Yb phase, becoming Al during subsequent high temperature aging3The core of the (Hf, Zr and Yb) composite particle is enriched with Zr and Hf elements with low diffusion rate in Al3An outer layer of Yb phase. Al (Al)3Yb promotes the desolventizing of Zr and Hf elements to minimize the solid solution degree of Zr and Hf in the alloy matrix, thereby achieving the purpose of improving the conductivity of the alloy, and Zr and Hf inhibit Al3The Yb particles are coarsened, and the purpose of improving the heat resistance of the alloy is further achieved. In addition, a proper amount of Hf element is matched with a proper amount of Zr element, the lower diffusion rate and the smaller atomic radius of Hf are utilized, the lattice distortion of solute atoms in an aluminum matrix and the mismatching degree of a precipitated phase interface are reduced, when the temperature is increased, the coarsening of a precipitated phase can be effectively inhibited, the resistance increasing effect caused by the thermal vibration of atoms is reduced, and the high-temperature conductivity of the alloy is improved.
The invention relates to a preparation process of a low-resistance temperature-sensitive high-conductivity heat-resistant aluminum alloy, which comprises the steps of remelting an industrial pure aluminum ingot with the purity of 99.7 percent, or adopting electrolytic aluminum liquid as an aluminum source, smelting at 760-780 ℃, adding an intermediate alloy, stirring, refining, quickly analyzing the components in front of a furnace after the intermediate alloy is molten, adjusting the components according to the designed material component ratio, keeping the temperature and standing at 710-730 ℃, and then casting and thermally treating to obtain an aluminum alloy ingot blank.
In the present invention, the aluminum source used is commercially pure aluminum. As a preferable scheme, the preparation process of the low-resistance temperature-sensitive high-conductivity heat-resistant aluminum alloy comprises the steps of preparing B element according to 0.02-0.10% of the total mass of the used industrial pure aluminum, adding the B element in the form of Al-B intermediate alloy before other intermediate alloys, stirring, standing, and then adding Al-Zr, Al-Hf and Al-Yb. When the content of Fe element in the industrial pure aluminum is lower than the designed content, adding Al-Fe intermediate alloy. As can be seen from FIGS. 2(a) and (B), the alloy of comparative example 6, to which no B element was added, contained more visible particles and coarse grains than the alloy of example 1 to which the Al-B master alloy was added during melting.
The invention relates to a preparation process of a low-resistance temperature-sensitive high-conductivity heat-resistant aluminum alloy, wherein the casting is rapid cooling casting, and the rapid cooling casting comprises but is not limited to water cooling casting; the cooling speed of the rapid cooling casting is 20-100 ℃/min; the ingot blank comprises a semi-continuous ingot and/or a continuous casting blank.
The preparation process of the low-resistance temperature-sensitive high-conductivity heat-resistant aluminum alloy comprises two-stage aging, wherein the first-stage aging temperature of the two-stage aging is 250-350 ℃, the heat preservation time is 4-8 hours, the second-stage aging temperature of the two-stage aging is 400-450 ℃, and the heat preservation time is 24-48 hours.
As can be seen by comparing FIG. 1(a) with FIG. 3, the alloy without the double-stage aging had extremely uneven precipitated phase size and coarsening phenomenon, and the precipitated phase particle size was larger than 50 nm.
The low-resistance temperature-sensitive high-conductivity heat-resistant aluminum alloy designed and prepared by the invention has the tensile strength of more than 70MPa, the conductivity at 20 ℃ of more than 60 percent IACS, the conductivity at 150 ℃ of more than 40 percent IACS and the conductivity at 200 ℃ of more than 36 percent IACS.
The low-resistance temperature-sensitive high-conductivity heat-resistant aluminum alloy designed and prepared by the invention has the strength residual rate of not less than 90 percent after heat preservation for 400 hours at 200 ℃ after cold deformation of 80 percent of deformation, namely the long-term heat-resistant temperature of not less than 200 ℃, and the strength residual rate of not less than 90 percent after heat preservation for 1 hour at 250 ℃, namely the short-term heat-resistant temperature of not less than 250 ℃.
The application of the low-resistance temperature-sensitive high-conductivity heat-resistant aluminum alloy designed and prepared by the invention comprises the steps of using the aluminum alloy as at least one of a guide rod, a bus and a lead; the guide rod is an anode guide rod for an aluminum electrolytic cell.
Drawings
FIG. 1(a) is a TEM bright field photograph of the alloy of example 2, FIG. 1(b) is a spectrum of a second phase of the alloy of example 2, and FIG. 1(c) is a TEM dark field photograph of the alloy of example 2;
FIG. 2(a) and FIG. 2(b) are metallographic photographs of comparative example 6 and example 1, respectively;
FIG. 3 is a TEM photograph of comparative example 5;
as can be seen from the TEM bright field image shown in FIG. 1(a), a large number of fine and dispersed second phase particles are precipitated in the alloy of example 2, and as can be seen from the energy spectrum shown in FIG. 1(b), the dispersed second phase particles are a composite phase containing Al, Hf, Zr and Yb, and as can be seen from the TEM dark field image shown in FIG. 1(c), Al having inner and outer layer contrast is formed3(Hf, Zr, Yb) composite particles having a particle size of less than 50 nm.
As can be seen from fig. 2(a) and 2(B), the alloy of comparative example 6, to which no B element was added, contained more visible particles and coarse grains than the alloy of example 1 to which the Al — B master alloy was added during melting.
As can be seen from FIG. 3, the alloy without the two-stage aging had very uneven precipitated phase size and coarsening, and the precipitated phase particle size was greater than 50 nm.
Detailed Description
In the examples and comparative examples, commercially pure aluminum ingots having a purity of more than 99.7%, Al-2.5% B master alloy, Al-5% Zr master alloy, Al-5% Hf master alloy, Al-10% Yb master alloy, and Al-9.3% Fe master alloy were used as raw materials. The preparation process comprises the following steps: melting industrial pure aluminum at 780 ℃, cooling to 740 ℃, preserving heat, adding an aluminum-boron intermediate alloy, stirring, standing, adding an aluminum-zirconium intermediate alloy, an aluminum-hafnium intermediate alloy and an aluminum-ytterbium intermediate alloy, adding an aluminum-iron intermediate alloy when the content of Fe element in the industrial pure aluminum is lower than the designed content of Fe element, stirring, refining, rapidly analyzing components in front of a furnace and adjusting the components after the intermediate alloy is completely melted, preserving heat at 720 ℃, standing for 10-15 min, and carrying out water cooling casting at the cooling speed of 30 ℃/min.
In examples 1 to 3 and comparative examples 1 to 5, the amount of the element B added during the smelting was 0.06% by mass of the commercially pure aluminum used.
In the comprehensive performance evaluation tables of examples and comparative examples, the tensile strength is measured after the alloy in an as-cast state is subjected to heat treatment; the heat-resistant temperature is measured after the heat-treated blank is subjected to cold deformation with 80% of deformation; the conductivity at 20 ℃ is tested according to GB/T12966-2008, the conductivity above 20 ℃ is measured by a four-point method, the sample is heated to a test temperature, and the resistivity is measured and calculated and converted into the conductivity.
In the products obtained in the inventive examples and comparative examples 1-5, the content of impurity Si is less than 0.05 wt%, and the sum of the contents of impurities Ti, V, Cr, Mn, etc. is less than 0.01 wt%. The sum of the contents of the impurity elements is less than 0.06 wt%.
Example 1
The mass percentage of each element after the components are adjusted is as follows: zirconium 0.10%, hafnium 0.03%, ytterbium 0.20%, iron 0.11%, and the balance of Al and inevitable impurity elements, rapidly cooling and casting, maintaining the temperature at 250 ℃ for 8 hours, then raising the temperature to 400 ℃ for 48 hours, and obtaining an aluminum alloy blank, wherein the measured comprehensive properties are shown in table 1.
Table 1 table of evaluation of comprehensive properties of example 1
Example 2
The mass percentage of each element after the components are adjusted is as follows: zirconium 0.05%, hafnium 0.02%, ytterbium 0.20%, iron 0.11%, and the balance of Al and inevitable impurity elements, rapidly cooling and casting, maintaining the temperature at 250 ℃ for 8 hours, then raising the temperature to 450 ℃ for 24 hours, obtaining an aluminum alloy blank, and measuring the comprehensive properties as shown in table 2.
Table 2 table of evaluation of comprehensive properties of example 2
Example 3
The mass percentage of each element after the components are adjusted is as follows: zirconium 0.05%, hafnium 0.01%, ytterbium 0.10%, iron 0.11%, and the balance of Al and inevitable impurity elements, rapidly cooling and casting, maintaining the temperature at 250 ℃ for 8 hours, then raising the temperature to 450 ℃ for 24 hours, obtaining an aluminum alloy blank, and measuring the comprehensive properties as shown in table 3.
Table 3 table for evaluating comprehensive properties of example 3
Comparative example 1
The mass percentage of each element after the components are adjusted is as follows: zirconium 0.18%, hafnium 0.02%, ytterbium 0.20%, iron 0.11%, and the balance of Al and inevitable impurity elements, to obtain an aluminum alloy blank, maintaining the temperature at 250 ℃ for 8 hours, then raising the temperature to 450 ℃ for 24 hours, and measuring the comprehensive properties as shown in Table 4.
Table 4 comprehensive performance evaluation table of comparative example 1
Comparative example 2
The mass percentage of each element after the components are adjusted is as follows: zirconium 0.05%, hafnium 0.15%, ytterbium 0.20%, iron 0.11%, and the balance of Al and inevitable impurity elements, to obtain an aluminum alloy billet, maintaining the temperature at 250 ℃ for 8 hours, then raising the temperature to 450 ℃ for 24 hours, and measuring the comprehensive properties as shown in table 5.
TABLE 5 comprehensive performance evaluation table of comparative example 2
It can be seen from comparative examples 1 and 2 that when either of the zirconium and hafnium components is outside the scope of the present invention, the conductivity of the resulting aluminum alloy is significantly reduced, which is far beyond the expectation, as compared to example 2.
Comparative example 3
The mass percentage of each element after the components are adjusted is as follows: zirconium 0.10%, hafnium 0.10%, ytterbium 0.20%, iron 0.11%, and the balance of Al and inevitable impurity elements, rapidly cooling and casting, maintaining the temperature at 250 ℃ for 8 hours, then raising the temperature to 400 ℃ for 48 hours, and obtaining aluminum alloy blanks, wherein the measured comprehensive properties are shown in table 6.
TABLE 6 comprehensive performance evaluation table of comparative example 3
When the total content of zirconium and hafnium is more than 0.15%, the electric conductivity of the obtained aluminum alloy is significantly decreased, as compared to example 1.
Comparative example 4
The mass percentage of each element after the components are adjusted is as follows: zirconium 0.05%, hafnium 0.02%, ytterbium 0.05%, iron 0.11%, and the balance of Al and inevitable impurity elements, rapidly cooling and casting, maintaining the temperature at 250 ℃ for 8 hours, then raising the temperature to 450 ℃ for 24 hours, obtaining an aluminum alloy blank, and measuring the comprehensive properties as shown in table 7.
TABLE 7 comprehensive performance evaluation Table for comparative example 4
When the mass ratio of ytterbium and zirconium is not more than 1, the strength and the electric conductivity of the obtained aluminum alloy are lower than those of the embodiment 2.
Comparative example 5
The mass percentage of each element after the components are adjusted is as follows: 0.05% of zirconium, 0.02% of hafnium, 0.20% of ytterbium, 0.11% of iron, and the balance of Al and unavoidable impurities, rapidly cooling and casting, and then annealing at 350 ℃ for 72 hours to obtain an aluminum alloy blank, wherein the measured comprehensive properties are shown in Table 8.
TABLE 8 comprehensive performance evaluation table of comparative example 5
The absence of the dual stage heat treatment reduces the electrical conductivity and heat resistance temperature of the alloy compared to example 2.
Comparative example 6
In the smelting process, aluminum-boron intermediate alloy is not added, and the mass percentage of each element after the components are adjusted is as follows: zirconium 0.05%, hafnium 0.02%, ytterbium 0.20%, iron 0.11%, and the balance of Al and unavoidable impurities, rapidly cooling and casting, maintaining the temperature at 250 ℃ for 8 hours, then raising the temperature to 450 ℃ for 24 hours, obtaining an aluminum alloy blank, and measuring the comprehensive properties as shown in Table 9.
TABLE 9 comprehensive performance evaluation Table for comparative example 6
Compared with the embodiment 2, the aluminum boron intermediate alloy is not added in the smelting process, the strength and the heat resistance are not greatly influenced, but the electric conductivity is reduced.

Claims (5)

1. A low resistance temperature sensitive high conductivity heat resistant aluminum alloy is characterized in that; the aluminum alloy comprises the following alloy elements in percentage by mass:
Zr :0.01~0.10%;
Hf: 0.01~0.10%;
Yb: 0.05~0.20%;
Fe :0.05~0.15%;
in the aluminum alloy, the mass ratio of Yb to Zr is more than 1, the total content of Zr and Hf is less than or equal to 0.15%, the content of impurity Si is less than 0.05%, and the total content of impurities Ti, V, Cr and Mn is less than 0.01%;
the aluminum alloy contains Al3(Hf, Zr, Yb) composite particles; the Al is3The core of the (Hf, Zr, Yb) composite particle is Al3Yb, Zr and Hf elements are enriched in Al3An outer layer of Yb particles; the Al is3The particle size of the (Hf, Zr, Yb) composite particles is less than 50 nm;
the low-resistance temperature-sensitive high-conductivity heat-resistant aluminum alloy is prepared by the following method:
remelting an industrial pure aluminum ingot with the purity of 99.7 percent, preparing B element according to 0.02-0.10 percent of the total mass of the used industrial pure aluminum, wherein the B element is added in the form of Al-B intermediate alloy before other intermediate alloys, the smelting temperature is controlled to be 760-780 ℃, and Al-Zr, Al-Hf and Al-Yb are added after stirring and standing, when the content of Fe element in the industrial pure aluminum ingot is lower than the designed content, the Al-Fe intermediate alloy is added into the intermediate alloy, after the intermediate alloy is melted, stirring, refining and rapid analysis of components before the furnace are carried out, the components are adjusted according to the designed material group distribution ratio, the temperature is kept to be 710-730 ℃, and then casting and heat treatment are carried out to obtain an aluminum alloy blank;
the casting is water-cooling casting; the ingot blank comprises a semi-continuous ingot or a continuous casting blank;
the heat treatment is double-stage aging; the first-stage aging temperature of the two-stage aging is 250-350 ℃, the heat preservation time is 4-8 h, the second-stage aging temperature of the two-stage aging is 400-450 ℃, and the heat preservation time is 24-48 h.
2. The low-resistance temperature-sensitive high-conductivity heat-resistant aluminum alloy according to claim 1, wherein: in the aluminum alloy, the mass ratio of Yb to Zr is 1.5-5: 1.
3. The low-resistance temperature-sensitive high-conductivity heat-resistant aluminum alloy according to claim 1, wherein:
the aluminum alloy comprises the following components in percentage by mass:
Zr :0.05~0.10%;
Hf :0.01~0.05%;
Yb :0.10~0.20%;
Fe :0.08~0.15%;
the content of impurity Si is less than 0.05%;
the total content of impurities Ti, V, Cr and Mn is less than 0.01 percent;
the balance being Al.
4. The low-resistance temperature-sensitive high-conductivity heat-resistant aluminum alloy according to claim 1, wherein: the prepared aluminum alloy has the conductivity of more than 60 percent IACS at 20 ℃, the conductivity of more than 40 percent IACS at 150 ℃, the conductivity of more than 36 percent IACS at 200 ℃, the long-term heat-resistant temperature of not less than 200 ℃ and the short-term heat-resistant temperature of not less than 250 ℃.
5. Use of the low-resistance temperature-sensitive high-conductivity heat-resistant aluminum alloy according to any one of claims 1 to 3, wherein: the application comprises using the material as at least one of a guide rod, a bus bar and a conducting wire; the guide rod is an anode guide rod for an aluminum electrolytic cell.
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